The first and second protonation constant (logβ111,logβ121) of the metal-ligand complex Gadolinium(III)-diethyltriamine-pentaacetic acid (DTPA) have been determined to be 2.27 and 1.52 at 25 °C and I = 0.1. A technique in which the three complexes (H2Gd-DTPA, HGd-DTPA−1, Gd-DTPA−2) are separated according to their relative polarity is utilized. An inductively coupled plasma-atomic emission spectrometer (ICP-AES) is used to determine the relative concentrations of each species by monitoring the gadolinium concentration.